CN114602332B - New concept molecular sieve membrane and preparation method and application thereof - Google Patents
New concept molecular sieve membrane and preparation method and application thereof Download PDFInfo
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- B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
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Abstract
The invention discloses a new concept molecular sieve membrane and a preparation method and application thereof. The invention breaks through the concept that the traditional molecular sieve must have intrinsic pores, and orderly assembles non-porous small organic molecular crystals without separation performance on the surface of an active layer by a simple and extremely high-repeatability method to form a fixed molecular transmission channel, thereby realizing excellent gas screening selectivity.
Description
Technical Field
The invention provides a new concept molecular sieve membrane and preparation and application thereof, belonging to the technical field of chemical separation.
Background
The membrane separation is an advanced substance separation technology, and has the characteristics of high efficiency, low energy consumption, environmental friendliness and the like, so that the membrane separation method is widely applied to the fields of chemical industry, medicine, water treatment and the like. Membrane separation is classified into ultrafiltration, microfiltration, nanofiltration and molecular sieving according to the separation principle. Wherein molecular sieving is a process of separating a group of molecules having a minute size difference, (e.g., H) 2 /CO 2 Separating, wherein the size difference is 0.04nm, which is equivalent to one hundred million of hair wiresAnd one) a first step. The separation difficulty is the greatest, and the requirements on membrane materials are the highest. Molecular sieve membranes reported in the current literature and patent publications are all constructed from microporous materials, such as zeolites, metal-organic frameworks, carbon materials, and porous organic frameworks. The molecular sieve membrane can enable small molecules to penetrate and large molecules to be intercepted, so that effective sieving of molecules with different sizes and shapes is realized. In summary, molecular sieve membranes have been reported to date, which are characterized in that: the membrane material must possess intrinsic pores with pore diameters in the range of from Emi to nanometer-! ZIF-8 membranes reported in the literature (Andrew J.Brown, nicholas A.Brunelli, kiwonEum, fereshteh Rashidi, J.R.Johnson, william J.Koros, christopher W.Jones, sankar Nair.2014,345, 72-75) which screen hydrogen and propane using 0.34nm intrinsic pores. Patent (CN 102974229 a) and patent (CN 105709610B) disclose an ultra-thin two-dimensional layered membrane material for hydrogen and carbon dioxide separation using a pore size of 0.21 nm.
Disclosure of Invention
The invention provides a new concept molecular sieve membrane, a preparation method and application thereof. The invention breaks through the concept that the traditional molecular sieve must have intrinsic pores, orderly assembles non-porous organic micromolecular crystals without separation performance on the surface of an active layer by a simple and extremely high-repeatability method to form a fixed molecular transmission channel, and realizes a group of molecules with small size difference, such as H 2 /CO 2 And (5) accurately screening. In order to achieve the aim of the invention, the invention adopts the following technical scheme:
the preparation method of the novel molecular sieve membrane comprises the following steps:
(1) Preparing active particles in advance;
ordered assembly of the nonporous organic small molecule crystals is carried out by the surface of the active particle layer. Wherein the active particles refer to metal particles, metal oxide particles, metal-organic framework particles, including but not limited to ZnO, MOF-74-M (M=Zn, mg, mn, co, ni, fe), ZIF-8, ZIF-67, ZIF-4, HKUST-1, MOP-1, MOF-5.
(2) Coating active particles on a supporting substrate (carrier) in advance but uniformly to form an active layer; wherein the ratio of the mass of the active particles to the diameter of the support substrate is 1-100mg:1-10cm.
Wherein the support substrate includes, but is not limited to, an alumina substrate, a stainless steel substrate, an anodized aluminum substrate, a silica substrate, a zirconia substrate, a titania substrate, a zinc oxide substrate, a nickel foam substrate, and the like. Wherein the coating method includes, but is not limited to, manual wiping, spraying, spin coating, hot pressing. In the membrane assembly process, the carrier is placed on a polytetrafluoroethylene support.
The morphology and size of the active particles are not limited, but particles of 10 to 100000nm are preferable. The net loading is 1-100mg (removal of solvent which may be included), preferably 10-30mg (removal of solvent which may be included).
(3) Heating a support carrier (the support substrate treated in the step (2)) in a closed non-porous small organic molecule crystal atmosphere, and sequentially assembling non-porous small organic molecule crystals without separation performance on the surface of an active layer to form a fixed molecule transmission channel;
wherein the assembly process is performed in a closed, heated, and organic small molecule crystal-containing environment.
Wherein the nonporous organic small molecule crystal (ligand) mainly refers to imidazoles or substituted derivatives thereof, pyrazines or substituted derivatives thereof, piperazines or substituted derivatives thereof, pyrimidines or substituted derivatives thereof, pyridazines or substituted derivatives thereof, carboxylic acid compounds, including but not limited to imidazole, 2-methylimidazole, benzimidazole, 2-nitroimidazole, 2-ethylimidazole, pyrazine, terephthalic acid, 2, 5-dihydroxyterephthalic acid.
Wherein the assembly process is performed in a reaction kettle.
Wherein the preparation and assembly (heating treatment) temperature is 80-500 ℃, preferably 100-400 ℃, the duration is 1-14400min, and the mass ratio of the organic small molecular crystal to the active particles is 10-5000:1, the pressure in the reaction kettle is 0.01-1MPa, preferably 0.03-0.2MPa.
It is still another object of the present invention to provide a novel concept molecular sieve membrane prepared by the above method.
It is also an object of the present invention to provide a novel concept molecular sieve membrane gas separation application utilizing supramolecular assembly for the separation of a set of molecules with small size differences (0.001 nm-1 nm).
Wherein a group of molecules includes but is not limited to H 2 /CO 2 ，H 2 /N 2 ，H 2 /CH 4 ，H 2 /C 3 H 8 ，H 2 /C 4 H 8 ，CO 2 /N 2 ，CO 2 /CH 4 ，C 2 H 4 /C 2 H 6 ，C 3 H 6 /C 3 H 8 。
The invention has the following effects and benefits: the invention breaks through the cognition of the traditional molecular sieve membrane, orderly assembles non-porous organic small molecular crystals without separation performance on the surface of the active layer, forms a fixed molecular transmission channel with the size at the nanometer level by virtue of intermolecular acting force, and realizes excellent gas sieving selectivity. The innovative preparation method is simple and easy to operate, low in cost, free of solvent pollution and good in repeatability. Has important significance for the field of membrane separation.
Drawings
The invention is shown in the accompanying figure 7:
FIG. 1 is a schematic diagram of a reaction apparatus ((1) a reaction vessel, (2) a polytetrafluoroethylene support, (3) a carrier, and (4) a ligand);
FIG. 2 is an X-ray diffraction pattern of the 2-methylimidazole film material and 2-methylimidazole powder material synthesized in example 1;
FIG. 3 is a scanning electron micrograph of the 2-methylimidazole film material synthesized in example 1;
FIG. 4 is a graph showing the permeability of hydrogen, methane, carbon dioxide, ethane, propane single component gases of the 2-methylimidazole membrane material synthesized in example 1;
FIG. 5 is a graph showing the ideal hydrogen/carbon dioxide, hydrogen/methane, hydrogen/ethane, hydrogen/propane selectivities of the 2-methylimidazole membrane materials synthesized in example 1;
FIG. 6 is the permeability of the hydrogen/carbon dioxide mixed gas of the 2-methylimidazole membrane material synthesized in example 1;
FIG. 7 shows the hydrogen/carbon dioxide mixed gas selectivity of the 2-methylimidazole membrane material synthesized in example 1.
Detailed Description
The following describes the embodiments of the present invention in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
Example 1.2 preparation of methylimidazole Membrane Material
Stainless steel substrates having a diameter of 2cm were immersed in nitrogen, dimethylformamide. And stirred at room temperature, wherein the stirring speed is 360 revolutions per minute, the stirring time is 60 minutes, and then the mixture is heated and dried in an oven at 60 ℃ for 720 minutes. 10mg of pre-prepared 100-500nmMOF-74-Zn seed (J.E.Bachman, Z.P.Smith, T.Li, T.Xu, J.R.Long.Enhanced ethylene separation and plasticization resistance in polymer membranes incorporating metal-organic framework nanocrystallites. Nat. Mater.15,845-849 (2016)) was then applied to the above treated stainless steel support by hand-wiping. The above-mentioned MOF-74-Zn seed coated support was fixed on a polytetrafluoroethylene support, which was then placed in a 100ml reaction kettle containing 3g of 2-methylimidazole solid. Then heated at 150℃for 13 hours to give a 2-methylimidazole film.
EXAMPLE 2 preparation of pyrazine film Material
Stainless steel substrates having a diameter of 2cm were immersed in nitrogen, dimethylformamide. And stirred at room temperature, wherein the stirring speed is 360 revolutions per minute, the stirring time is 60 minutes, and then the mixture is heated and dried in an oven at 60 ℃ for 720 minutes. 10mg of pre-prepared 100-500nm MOF-74-Zn seed crystals (J.E.Bachman, Z.P.Smith, T.Li, T.Xu, J.R.Long.Enhanced ethylene separation and plasticization resistance in polymer membranes incorporating metal-organic framework nanocrystallisms. Nat. Mater.15,845-849 (2016)) were then applied to the above treated stainless steel support by hand-rubbing. The above-described MOF-74-Zn seed coated support was fixed to a self-made polytetrafluoroethylene support, which was then placed in a 100ml reactor containing 3g of pyrazine solid. Then, the mixture was heated at 130℃for 13 hours to obtain a pyrazine film.
Example 3.2 preparation of methylimidazole Membrane Material
By means of the nitrogen, the nitrogen is used,the nitrogen dimethylformamide was immersed in a stainless steel substrate having a diameter of 3 cm. And stirred at room temperature, wherein the stirring speed is 360 revolutions per minute, the stirring time is 60 minutes, and then the mixture is heated and dried in an oven at 60 ℃ for 720 minutes. Then 20mg of ZIF-8 seed crystal (Jia Xiao, kaidi Diao, zhou Zheng, xudong cui. MOF-derived porous ZnO/Co) prepared in advance and having a particle diameter of about 300nm was used 3 O 4 nanocomposites for high performance acetone gas send. Journal of Materials Science: materials in Electronics,29,8535-8546 (2018)) was applied to the treated stainless steel support by manual rubbing. The above ZIF-8 seed coated support was fixed to a polytetrafluoroethylene support and then placed in a 100ml reactor containing 3g of 2-methylimidazole solid. Then heated at 130℃for 13 hours to give a 2-methylimidazole film.
EXAMPLE 4 preparation of terephthalic acid film Material
Stainless steel substrates 5cm in diameter were immersed in nitrogen, dimethylformamide. And stirred at room temperature, wherein the stirring speed is 360 revolutions per minute, the stirring time is 60 minutes, and then the mixture is heated and dried in an oven at 60 ℃ for 720 minutes. Then 50mg of a pre-prepared MOF-5 seed crystal (Menghu Cai, liuying Qin, longtai You, yu Yao, huimin Wu, zhiqin Zhang, lu Zhang, xinghin Yon, jian Ni. Functionalization of MOF-5with monosubstituents:effects on drug delivery behavior.RSC Adv, 2020,10,36862) having a particle diameter of about 100nm was applied to the above-treated stainless steel support by a manual rubbing method. The above-described MOF-5 seed coated support was mounted on a polytetrafluoroethylene support, which was then placed in a 100ml reactor containing 5g terephthalic acid solids. Then heated at 400℃for 10 hours to obtain a terephthalic acid film.
FIG. 1 is a schematic view of a reaction device, as shown in FIG. 1, a molecular sieve membrane is prepared in a reaction kettle (1), a polytetrafluoroethylene support is placed in the reaction kettle (1), a support substrate coated with active particles is fixed on the polytetrafluoroethylene support, a nonporous small organic molecule crystal is placed below the polytetrafluoroethylene support, and the support carrier is subjected to heat treatment in the nonporous small organic molecule crystal atmosphere. FIG. 2 shows an X-ray diffraction pattern of the 2-methylimidazole film/powder material synthesized in example 1, with distinct characteristic peaks. FIG. 3 is a scanning electron micrograph of the 2-methylimidazole film material synthesized in example 1, showing a dense structure. FIG. 4 shows the permeability of hydrogen, methane, carbon dioxide, ethane and propane of the 2-methylimidazole membrane material synthesized in example 1, wherein the hydrogen permeability is obviously different from other gases. Fig. 5 shows the ideal selectivity of the 2-methylimidazole membrane materials synthesized in example 1 for hydrogen/carbon dioxide, hydrogen/methane, hydrogen/ethane, and hydrogen/propane, and shows good separation performance for hydrogen/carbon dioxide, hydrogen/methane, hydrogen/ethane, and hydrogen/propane. FIG. 6 is the permeability of the hydrogen/carbon dioxide mixed gas of the 2-methylimidazole membrane material synthesized in example 1. FIG. 7 shows the hydrogen/carbon dioxide mixed gas selectivity of the 2-methylimidazole membrane material synthesized in example 1. In general, the novel molecular sieve membrane material prepared by the method has excellent gas permeability and selectivity.
Claims (7)
1. The preparation method of the molecular sieve membrane is characterized by comprising the following steps:
(1) Coating active particles on a support substrate;
wherein the active particles are MOF-74-Zn;
(2) Under the airtight condition, heating the support substrate treated in the step (1) in the atmosphere of the nonporous small organic molecule crystal;
wherein the temperature of the heating treatment is 150 DEG C o C, heating treatment time is 13 hours, and the mass ratio of the organic small molecular crystal to the active particles is 300:1, a step of; the nonporous small organic molecule crystal is 2-methylimidazole.
2. The method according to claim 1, wherein the active particles have a particle diameter of 100 to 500 nm.
3. The preparation method according to claim 1, wherein the support substrate is one or more of an alumina substrate, a stainless steel substrate, an anodized alumina substrate, a silica substrate, a zirconia substrate, a titania substrate, a zinc oxide substrate, and a foam nickel substrate; the coating method is one or more of a manual wiping method, a spraying method, a spin coating method and a hot pressing method.
4. The method of claim 1, wherein the ratio of the mass of the active particles to the diameter of the support substrate is 10mg:2cm; the net loading of Zn in the MOF-74-Zn was 10mg.
5. A molecular sieve membrane made by the method of any one of claims 1-4.
6. The use of a molecular sieve membrane as claimed in claim 5 in gas separation.
7. The use according to claim 6, wherein the gas is H 2 /CO 2 ，H 2 /N 2 ，H 2 /CH 4 ，H 2 /C 3 H 8 ，H 2 /C 4 H 8 ，CO 2 /N 2 ，CO 2 /CH 4 ，C 2 H 4 /C 2 H 6 Or C 3 H 6 /C 3 H 8 。
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